MgO-Al_2O_3-SiO_2透明微晶玻璃结构与性能的研究
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摘要
MgO-Al2O3-SiO2(MAS)系统微晶玻璃具有优异的介电性能、机械性能、较好的化学稳定性、较低的热膨胀系数,使得其应用领域广阔,具有十分重要的科学研究意义。本文以MgO-Al2O3-SiO2系统微晶玻璃为研究对象,采用XRD、DSC、FE-SEM,热膨胀仪、高温旋转粘度仪、UV-Vis-NIR等测试手段,探索MAS系统透明微晶玻璃的组成——工艺——结构——性能之间的关系。首先,研究了晶核剂配比对MAS微晶玻璃结构和性能的影响,确定了合理的晶核剂组成及制备透明微晶玻璃合理的热处理制度。然后,对MAS微晶玻璃中引入一定量的碱土金属及碱金属,降低MAS微晶玻璃熔制难度,改善微晶玻璃性能。最后,通过对MAS微晶玻璃中掺杂稀土离子,探索了稀土离子对其物理性能、成核、析晶性能以及光透过性能的影响。通过上述实验,结果表明：
使用5%TiO2+3%ZrO2(wt%,下同)是制备MAS透明微晶玻璃较为合理的晶核剂配比。该晶核剂配比的基础玻璃在800℃/4h+950℃/1.5h热处理,可得到以尖晶石为主晶相,可见光透过率达到86%的接近无色透明的微晶玻璃,其平均晶粒尺寸为34nm。单独使用8%TiO2作为晶核剂时,在800℃/4h+950℃/1.5h热处理得到的微晶玻璃含MgTi2O5、MgAl2O4两种晶相,呈蓝紫色且可见光透过率达到83%。单独使用3-8%ZrO2作为晶核剂时,仅有含8%/ZrO2的MAS玻璃在900℃/6h+1060℃/6h热处理后得到了无色透明微晶玻璃,其主晶相为堇青石,但其熔制难度很大。
用0～4%的ZnO部分取代MAS玻璃中的MgO,采用二步法热处理制度800℃/4h+950℃/1.5h制备了透明微晶玻璃,其主晶相均为立方晶系的尖晶石晶体,随着ZnO含量增加,锌尖晶石比例逐渐增加。当ZnO取代量在0～3%时,MAS微晶玻璃在可见光区透过率均大于85%；但是当ZnO含量增加至4%时,微晶玻璃在可见光区透过率下降至79%。在紫外光波段,随着ZnO的量增加,紫外截止波长逐渐向短波方向移动。其中加入2%的ZnO就能显著细化晶粒尺寸、并使晶粒均匀分布,此时透明微晶玻璃平均晶粒尺寸仅为29.4nm,晶粒尺寸标准偏差为7.5。当ZnO取代MgO的量为2%～4%时,MAS微晶玻璃在800℃/4h+1000℃/1.5h热处理仍能保持外观透明。
将MAS玻璃中碱金属的含量控制在2%,分别用0.5%,1.0%,1.5%及2%的Li20代替MAS玻璃中Na2O,玻璃粘度先降低后升高,在取代量为1%时,降低高温粘度效果最明显,熔制温度最低。比较含2%Na2O、1%Li2O+1%Na2O及1%K20+1%Na20三种玻璃样品的粘度及析晶性能,其粘程活化能分别为306.04kJ/mol、284.01kJ/mol、288.78kJ/mol,熔制温度为1612-C、1508℃、1573℃。与仅含2%Na2O的玻璃样品相比,1%Li20的引入使MAS玻璃晶体的生长方式由二维析晶向整体析晶转变,同时主晶相变为石英固溶体,但对析晶活化能影响较小；1%K20的引入将MAS玻璃的析晶活化能由370.1kJ mo1-1降低为275.3kJmo1-1,而对晶化指数改变较小,该组成在880℃～1000℃的晶化温度范围内均能获得以尖晶石为主晶相的透明微晶玻璃。
在含1%Li20的MgO-Al2O3-SiO2中掺杂0-0.015mo1的Y203,随着Y203掺杂量增加,对MAS玻璃的玻璃转变温度几乎没有影响,膨胀软化温度由791℃增加至814-C,热膨胀系数由41×10-7/℃增加至45×10-7/℃,显微硬度由605kg/mm2增加至652kg/mm2。随着Y203含量的增加,对玻璃析晶的抑制作用越明显。当Y203的掺杂量为0～0.01mol时,MAS玻璃在840℃～1120℃晶化时均析出石英固溶体晶相(β-/α-quartz solid solution),在高于1000℃晶化时,主晶相p-石英固溶体在冷却过程中产生相变,成为α-石英固溶体。Y2O3掺杂量为0.015mo1的MAS玻璃样品在840℃晶化时保持为非晶态固体,在940℃-1120℃晶化时才有大量的石英固溶体晶相出现,在1060℃以上晶化开始观察到石英固溶体的相转变现象。掺杂Y203的量为0.005与0.01mol的样品在840℃晶化保温1.5h后外观透明,但透过率较低仅为41%。
Magnesium aluminosilicate (MAS) glass-ceramics containing spinel and high-/low quartz solid solution, own good chemical stability, low thermal expansion coefficient, excellent dielectrical property and good mechanical properties. In the dissertation, the compositions, processes, structure and properties of MAS glass-ceramics were investigated by XRD, DSC, horizontal dual-rod dilatometer, rotating crucible viscometer FE-SEM and UV-Vis-NIR. The results show that:
The MAS glass with5%TiO2+3%ZrO2(wt%, the same as below) as nucleating agents is reasonable to prepare transparent glass-ceramic. When nucleated at800℃for4h and then crystallized at950℃for1.5h, the nearly colorless transparent glass-ceramic with spinel as the main crystal phase was prepared, and the transmittance in the visible spectra region reached86%. The mean particle size of the transparent glass-ceramic was about34nm. As the MAS glass using only TiO2as nucleating agent, the prepared transparent glass-ceramic, containing MgTi2O5and MgAl2O4crystalline phases, was slight purple and with83%transmittance in visible spectra region. As using3-8%ZrO2as nucleating agent, only the ZrO2concentration reached8%, the transparent glass-ceramics could prepared by nucleated at900℃for6h and then crystallized at1060℃for6h. The glass-ceramic was absolutely colorless and with indialite as the main crystal phase. It could not be ignored that this compostion glass was difficult to melt, high temperature and long time to heat-treat.
In the MgO-Al2O3-SiO2system glass, the0～4%ZnO was partially substituted for MgO. The transparent glass-ceramics were prepared after two-step heat-treated schedule800℃/4h+950℃/1.5h, and the main crystal phase were spinel solid solution. With the increasing of ZnO content, the proportion of gahnite in the spinel solid solution increased. Meanwhile, the prepared MAS glass-ceramics were all with over85%transmittance in visible spectra region when the substitution content below3%. However, when the ZnO content increased to4%, the transmittance of glass-cermamic decreased to79%. In the UV spectral region, the UV cut-off wavelength shifted to the short wavelength direction with the increasing ZnO content.When the ZnO content was equal or greater than2%, it was effective to refine crystal size and make the gains uniformly distribution. The mean grain size of the glass-ceramics containg2%ZnO was only29.4nm, and the Sd was7.5. And the MAS glass-ceramics kept transparent even heat-treated800℃/4h+1000℃/1.5h. As to the same composition MAS glss-ceramic, the UV cut-off wavelength moved towards long wavelength with the increasing of crystallization temperature.
The effects of alkali metal oxide on the viscosity and crystallization properties of MAS glass-ceramics were studied. The primary MAS glass contained2%Na20, and the0.5%,1.0%,1.5%and2%Li2O were used to substitute for Na2O. The results showed that the viscosities of MAS glasses first decreased and then increased with the increasing of the Li2O-concentrations. As1%Na2O was replaced by the Li2O, the MAS glass had the lowest viscosity and melting temperature. The activation energy for viscous flow of MAS glass with2%Na2O,1%Li2O+1%Na2O,1%K20+1%Na20were306.04kJ/mol、284.01kJ/mol、288.78kJ/mol respectively, and the melting temperature were1612℃,1508℃,1573℃respectively. As compared to the glass containing2%Na2O, the introduction of Li2O changed the crystal phase precipitation mode from two-dimensional to bulk crystallization, but had little effect on the activation energy of crystallization. It also changed the main crytal phase to the quartz solid solution. The introduction of K2O decreased the activation energy of crystallization from370.1kJ mol-1to275.3kJ mol-1, but had little effect on the crystal phase precipitation mode. The MAS glass containing1%K2O+1%Na2O could prepare the transparent glass ceramic at the crystallization temperature range from880℃to1000℃.
The effects of Y2O3on the physical and crystallization properties of MgO-Al2O3-SiO2glass were investigated. As the Y2O3-concerntration grows from0to1.5mol%, the transformation temperature (Tg) varied slightly, the dilatometric softening temperature (Ts) increased from791℃to814℃, the CTE increased from41×10-7/℃to45×10-7/℃, and the micro hardness increased from605kg/mm2to652kg/mm2. The MAS glasses with0～0.01mol yttria precipitated the quartz solid solution when crystallized at the temperatures range from840℃to1120℃. As the glass was crystallized above1000℃, the high-to low quartz solid solution phase transformation was occured during the glass-ceramic cooling. The MAS glass doped with0.015mol Y2O3was still amorphous when heat-treated at840℃, at940℃～1120℃, the quartz solid solution phase presented, and at1060℃the phase transition of the high-to low-quartz solid solution was observed. The MAS glass doped with0.005mol and O.Olmol Y2O3were transparent with the transmittance about41%after heat-treated at840℃for1.5h.
使用5%TiO2+3%ZrO2(wt%,下同)是制备MAS透明微晶玻璃较为合理的晶核剂配比。该晶核剂配比的基础玻璃在800℃/4h+950℃/1.5h热处理,可得到以尖晶石为主晶相,可见光透过率达到86%的接近无色透明的微晶玻璃,其平均晶粒尺寸为34nm。单独使用8%TiO2作为晶核剂时,在800℃/4h+950℃/1.5h热处理得到的微晶玻璃含MgTi2O5、MgAl2O4两种晶相,呈蓝紫色且可见光透过率达到83%。单独使用3-8%ZrO2作为晶核剂时,仅有含8%/ZrO2的MAS玻璃在900℃/6h+1060℃/6h热处理后得到了无色透明微晶玻璃,其主晶相为堇青石,但其熔制难度很大。
用0～4%的ZnO部分取代MAS玻璃中的MgO,采用二步法热处理制度800℃/4h+950℃/1.5h制备了透明微晶玻璃,其主晶相均为立方晶系的尖晶石晶体,随着ZnO含量增加,锌尖晶石比例逐渐增加。当ZnO取代量在0～3%时,MAS微晶玻璃在可见光区透过率均大于85%；但是当ZnO含量增加至4%时,微晶玻璃在可见光区透过率下降至79%。在紫外光波段,随着ZnO的量增加,紫外截止波长逐渐向短波方向移动。其中加入2%的ZnO就能显著细化晶粒尺寸、并使晶粒均匀分布,此时透明微晶玻璃平均晶粒尺寸仅为29.4nm,晶粒尺寸标准偏差为7.5。当ZnO取代MgO的量为2%～4%时,MAS微晶玻璃在800℃/4h+1000℃/1.5h热处理仍能保持外观透明。
将MAS玻璃中碱金属的含量控制在2%,分别用0.5%,1.0%,1.5%及2%的Li20代替MAS玻璃中Na2O,玻璃粘度先降低后升高,在取代量为1%时,降低高温粘度效果最明显,熔制温度最低。比较含2%Na2O、1%Li2O+1%Na2O及1%K20+1%Na20三种玻璃样品的粘度及析晶性能,其粘程活化能分别为306.04kJ/mol、284.01kJ/mol、288.78kJ/mol,熔制温度为1612-C、1508℃、1573℃。与仅含2%Na2O的玻璃样品相比,1%Li20的引入使MAS玻璃晶体的生长方式由二维析晶向整体析晶转变,同时主晶相变为石英固溶体,但对析晶活化能影响较小；1%K20的引入将MAS玻璃的析晶活化能由370.1kJ mo1-1降低为275.3kJmo1-1,而对晶化指数改变较小,该组成在880℃～1000℃的晶化温度范围内均能获得以尖晶石为主晶相的透明微晶玻璃。
在含1%Li20的MgO-Al2O3-SiO2中掺杂0-0.015mo1的Y203,随着Y203掺杂量增加,对MAS玻璃的玻璃转变温度几乎没有影响,膨胀软化温度由791℃增加至814-C,热膨胀系数由41×10-7/℃增加至45×10-7/℃,显微硬度由605kg/mm2增加至652kg/mm2。随着Y203含量的增加,对玻璃析晶的抑制作用越明显。当Y203的掺杂量为0～0.01mol时,MAS玻璃在840℃～1120℃晶化时均析出石英固溶体晶相(β-/α-quartz solid solution),在高于1000℃晶化时,主晶相p-石英固溶体在冷却过程中产生相变,成为α-石英固溶体。Y2O3掺杂量为0.015mo1的MAS玻璃样品在840℃晶化时保持为非晶态固体,在940℃-1120℃晶化时才有大量的石英固溶体晶相出现,在1060℃以上晶化开始观察到石英固溶体的相转变现象。掺杂Y203的量为0.005与0.01mol的样品在840℃晶化保温1.5h后外观透明,但透过率较低仅为41%。
Magnesium aluminosilicate (MAS) glass-ceramics containing spinel and high-/low quartz solid solution, own good chemical stability, low thermal expansion coefficient, excellent dielectrical property and good mechanical properties. In the dissertation, the compositions, processes, structure and properties of MAS glass-ceramics were investigated by XRD, DSC, horizontal dual-rod dilatometer, rotating crucible viscometer FE-SEM and UV-Vis-NIR. The results show that:
The MAS glass with5%TiO2+3%ZrO2(wt%, the same as below) as nucleating agents is reasonable to prepare transparent glass-ceramic. When nucleated at800℃for4h and then crystallized at950℃for1.5h, the nearly colorless transparent glass-ceramic with spinel as the main crystal phase was prepared, and the transmittance in the visible spectra region reached86%. The mean particle size of the transparent glass-ceramic was about34nm. As the MAS glass using only TiO2as nucleating agent, the prepared transparent glass-ceramic, containing MgTi2O5and MgAl2O4crystalline phases, was slight purple and with83%transmittance in visible spectra region. As using3-8%ZrO2as nucleating agent, only the ZrO2concentration reached8%, the transparent glass-ceramics could prepared by nucleated at900℃for6h and then crystallized at1060℃for6h. The glass-ceramic was absolutely colorless and with indialite as the main crystal phase. It could not be ignored that this compostion glass was difficult to melt, high temperature and long time to heat-treat.
In the MgO-Al2O3-SiO2system glass, the0～4%ZnO was partially substituted for MgO. The transparent glass-ceramics were prepared after two-step heat-treated schedule800℃/4h+950℃/1.5h, and the main crystal phase were spinel solid solution. With the increasing of ZnO content, the proportion of gahnite in the spinel solid solution increased. Meanwhile, the prepared MAS glass-ceramics were all with over85%transmittance in visible spectra region when the substitution content below3%. However, when the ZnO content increased to4%, the transmittance of glass-cermamic decreased to79%. In the UV spectral region, the UV cut-off wavelength shifted to the short wavelength direction with the increasing ZnO content.When the ZnO content was equal or greater than2%, it was effective to refine crystal size and make the gains uniformly distribution. The mean grain size of the glass-ceramics containg2%ZnO was only29.4nm, and the Sd was7.5. And the MAS glass-ceramics kept transparent even heat-treated800℃/4h+1000℃/1.5h. As to the same composition MAS glss-ceramic, the UV cut-off wavelength moved towards long wavelength with the increasing of crystallization temperature.
The effects of alkali metal oxide on the viscosity and crystallization properties of MAS glass-ceramics were studied. The primary MAS glass contained2%Na20, and the0.5%,1.0%,1.5%and2%Li2O were used to substitute for Na2O. The results showed that the viscosities of MAS glasses first decreased and then increased with the increasing of the Li2O-concentrations. As1%Na2O was replaced by the Li2O, the MAS glass had the lowest viscosity and melting temperature. The activation energy for viscous flow of MAS glass with2%Na2O,1%Li2O+1%Na2O,1%K20+1%Na20were306.04kJ/mol、284.01kJ/mol、288.78kJ/mol respectively, and the melting temperature were1612℃,1508℃,1573℃respectively. As compared to the glass containing2%Na2O, the introduction of Li2O changed the crystal phase precipitation mode from two-dimensional to bulk crystallization, but had little effect on the activation energy of crystallization. It also changed the main crytal phase to the quartz solid solution. The introduction of K2O decreased the activation energy of crystallization from370.1kJ mol-1to275.3kJ mol-1, but had little effect on the crystal phase precipitation mode. The MAS glass containing1%K2O+1%Na2O could prepare the transparent glass ceramic at the crystallization temperature range from880℃to1000℃.
The effects of Y2O3on the physical and crystallization properties of MgO-Al2O3-SiO2glass were investigated. As the Y2O3-concerntration grows from0to1.5mol%, the transformation temperature (Tg) varied slightly, the dilatometric softening temperature (Ts) increased from791℃to814℃, the CTE increased from41×10-7/℃to45×10-7/℃, and the micro hardness increased from605kg/mm2to652kg/mm2. The MAS glasses with0～0.01mol yttria precipitated the quartz solid solution when crystallized at the temperatures range from840℃to1120℃. As the glass was crystallized above1000℃, the high-to low quartz solid solution phase transformation was occured during the glass-ceramic cooling. The MAS glass doped with0.015mol Y2O3was still amorphous when heat-treated at840℃, at940℃～1120℃, the quartz solid solution phase presented, and at1060℃the phase transition of the high-to low-quartz solid solution was observed. The MAS glass doped with0.005mol and O.Olmol Y2O3were transparent with the transmittance about41%after heat-treated at840℃for1.5h.
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